Process of purifying graphite.



PATENTED AUG. 1a,, 1903.

'M. F. R. GLOGNBR. PROCESS OF PURIFYING GRAPHITE.

APPLIOATION TILED JAN. 27. 1903.

N0 MODEL.

Wit passes- 17%.

An-mpys rm: mums vzrzns on PHOTO-LITNO., WASHINGTON, w. c.

NITED STATES Patented August 18, 19Q3.

ATENT IFFIcE.

PROCESS OF PURlFYlNG GRAPHITE.

SPECIFICATION forming part of Letters Patent No. 736,381, dated August18, 1903.

Application filed January 27,1903. Serial No. 140,786. (No specimens.)

1'0 (0M w/tom it may concern.-

Be it known that I, MORITZ FRIEDRICH REINHOLD GLoeNER, a subject of theKing of Prussia, German Emperor, residing at Freiburg, in the Kingdom ofPrussia, German Empire,have invented certain new and useful Improvementsin Processes of Purifying Graphite; and I do hereby declare that thefollowing is a full, clear, and exact description,

The present invention relates to a process for purifying graphite fromits natural mineral impuritiesfihich process is especially adapted to becarried out on a manufacturing scale,because, on the one hand, it isvery simple and cheap,and, on the other hand,the final result is verygood and far superior to any obtainable by processes hitherto employed.

In my new process after being purified in afirst washfrom its heavierimpuritiesas, for instance, quartz,-iron, and the likeby means of coldwater the graphite mineral is mixed with about three or four times itsweight of water to a thin paste. A quantity of petroleum is then addedto this paste, which quantity is about half as much as the amount ofpure graphite contained in the graphite mixture, and the whole isthoroughly stirred within a closed vessel. Afterward the vessel isallowed to stand, and water is sprinkled over the surface of the liquidby means of a rose or the like in order to obtain a quicker and morecomplete separation of the graphite particlesfrom the earthy admixtures.

'In my present invention I desire first to point out that the graphitemixture as submitted to the process of purification by means of waterand petroleum consists, exclusively, of graphite and earthy admixtures.Only by this means is the quick and complete purification of thegraphite by means of the subsequent treatment rendered possible. If thegraphite were to be purified by means of water and petroleum while theheavier admixtures are still present, a far greater amount of petroleum,as well as of labor, would be necessary, yet a complete separation ofthe graphite from its admixtures would be impossible. The productobtained thus would not be pure. The high degree of purity, however,determines the value of the product.

For carrying out my new process preferably a plurality of agitating orshaking devices are arranged close to each other, one Workman beingsufficient for attending four of them.

Figure 1 of the accompanying drawings illustrates two agitating devicesarranged close to each other, one apparatus being shown in elevation andthe other in a section on line 1 l in Fig. 2. Fig. 2 represents alongitudinal section of an agitating apparatus.

Each agitator A is obliquely suspended on three chains 13 in such amanner that the Wave formed when the vessel is agitated falls back onthe higher part of-the bottom and a thorough mixing of oil and graphiteis obtained, the operation being at the same time facilitated. Eachvessel A has a handle 0.

a is graphite filled in a wet state. 7

b is the water with the layer of oil.

0 c are covers.

dis an outlet-hole for the pulpy residuefor instance, a hand-hole with acover, a door, or the like. The tubefis in connection with awater-supply g and fitted with a flexibletube h and a rose 2'. The tubeis connected with an oil-supply Z and also fitted with a flexible tubem, leading to a mouthpiece 'n.

The devices are preferably operated by human force, because thetreatment of the material is utterly difficult, and a throughout specialtreatment is required for each of the large number of varieties of thematerial.

Before the graphite is brought into the vessels A it is separated fromits heavier admixtures-as quartz, iron, and the like-which in the wellknown manner is efi'ectedl by washing the material with water in longkennels. Exactly weighted quantities of the material which thus containsonly graphite and earthy admixtures are brought into the vessels A.Then, first'water is admitted from the tube h and later oil from thetube m.

The vessels A are agitated in short shocks, about thirty per minute.After the agitation has taken place the mixture of oil and graphitefloating at the surface is subjected to a uniform action of the rose,whereafter the vessel is allowed to stand in order to obtain theseparation of the earthy parts. After the attendant has operated fouragitators in the described manner the dirty water in the first vesselhas become clear in the meautime. The workman takes off: the oil-graphite and puts it into a collector for the further treatment in order toobtain in any wellknown manner a separation of the oil from thegraphite.

The mixture containing only fine earthy substances and graphite is mixedwith a quantity of water the weight of which is about three or fourtimes as great as that of the graphite mixture. Petroleum is then addedin the approximate proportion of one part petroleum to two parts ofgraphite contained in the mixture. Now the whole is given a strongrotating, rocking, or reciprocating movement within a closed vessel, sothat the mixture is thoroughly stirred and intimately mingled.The'petroleum is broken up into very fine drops or perles, and everygraphite particle when touching them is attracted, while the earthyparticles, which were already saturated with water before the additionof petroleum,remain completely neutral. After the Vessel has beenallowed to stand the earthy parts sink down, while the petroleumcarrying the graphite tends to rise to the surface. After a certain timewater is then sprinkled over the surface of the liquid by means of arose or the like, whereby the fine earthy particles are caused to sinkmore quickly, and any earthy particles which may be carried upward bythe rising petroleum and froth are caused to sink down again.

The vessel is shaken once, twice, or repeatedly after the graphite hasbeen skimmed, and every time some petroleum is added. The whole of thegraphite will then be taken off by the petroleum.

In the described manner the graphite is quickly, well, and cleanlyseparated from its earthy admixtures. The product obtained is of bestquality and purity, yet the amount of petroleum and labor needed isinsignificant. It is even rendered possible by my process to workgraphite mixtures which only contain ten per cent. graphite and toobtain from them a product which is as valuable as the Ceylon graphite.

My new process is furthermore especially adapted for the purification ofthe small dense crystalline varieties of graphite, for which acommercial purifying process has not existed up to the present time.

Having now described my invention and in what manner the same is to beperformed,

what I claim, and desire to secure by Letters Patent, is

A process for purifying graphite in a wet and cold manner by the use ofwater and petroleum, consisting in the following operations: purifyingthe graphite mineral from its heavy admixtures (as for instance quartz,iron and the like) by a washing with cold water; mixing said purifiedgraphite mineral with about three or four times its weight of coldwater; very strongly agitating said paste within a closed vessel afterthe addition of a quantity of petroleum of about half the weight of thepure graphite contained in the mixture; and then sprinkling water overthe surface of the liquid, after the mixture has been allowed to stand,in order to obtain a quicker and more complete separation of thegraphite particles from the earthy substances, substantially asdescribed.

In witness whereofI have hereunto set my hand in presence of twowitnesses.

MORITZ FREIDRICI-l REINIIOLD GLOGNER.

Witnesses:

ERNST. KRATZ, ALBERT SOHENK.

